Portable Carbon Dioxide Supercritical Fluid Extraction Prototype

by

Ritthikiat Churoop 5810545327

Phanuwat Chaichutchouwakul 5910546163

A senior project submitted in partial fulfillment of the

requirement for the degree of

Bachelor of Engineering
(Mechanical Engineering)

at the

Department of Mechanical Engineering

Faculty of Engineering
Kasetsart University
2019
 Scan here

For Digital Content

 Portable Carbon Dioxide Supercritical Fluid Extraction Prototype
by

Ritthikiat Churoop 5810545327

Phanuwat Chaichutchouwakul 5910546163

Mechanical Engineering Project

Department of Mechanical Engineering
Faculty of Engineering
Kasetsart University

A senior project submitted in partial fulfillment of the requirement for the

degree of Bachelor of Engineering
(Mechanical Engineering)

Approved by

Senior Project Adviser: ………………………………….……………..……..............Date:………...........

(Assistant Professor Taweedej Sirithanaphiphat, Ph.D.)

Project Committee: .................................................................................Date:....................

(Ajarn Varodom Toochinda, Ph.D.)
Ritthikiat Churoop, Phanuwat Chaichutchouwakul
Academic Year 2019
Carbon Dioxide Supercritical Fluid Extraction Prototype
Bachelor of Engineering (Mechanical Engineering)
Department of Mechanical Engineering, Faculty of Engineering, Kasetsart University

Abstract

Supercritical fluid extraction (SFE) has become one of the most popular
extraction techniques, nowadays since it has demonstrated many advantages
compared with traditional or classical extraction processes. Aspects such as improved
selectivity, higher extraction yields, better fractionation capabilities, and lower
environmental impacts have been crucial to the important growth of SFE. The
fundamentals of SFE are shown together with the most important variables that can
affect the extraction process for each material and their tuning process. The cost of
extractor is very expensive, fixed extractor (unmovable). Because most of machines
are recirculate CO2 which has more components such as separator, pump, the
controller and it need to import from abroad. So, we attempt to make it portable and
localize (use AISI 1024 as material and non-circulated carbon dioxide) in this project.
Based on high pressure vessel design. The extractor prototype volume is 800 ml it can
load solid carbon dioxide 400 g – 500 g and raw material 50 g. From the experiment
we can heat to change phase from solid to supercritical point and also can control
temperature inside vessel (0 – 120 °C) and pressure (40 Bar - 220 Bar) before leak at
125 °C and 230 Bar. The defect is not from high-pressure vessel design but from the
deformation of rubber O – ring (the rubber O – ring can resist at temperature 100 °C
and pressure 200 Bar) that cannot resist. The prototype is able to extract the oil but
don’t know how to collect the oil in correct ways because when relieving the pressure
inside the vessel, carbon dioxide (gas) will carry the oil out but some remains on valve
surface and inside the vessel so the evidence of the oil are in the form of scent.
Key Word: Extraction Method, Super Critical Fluid Extraction, Essential Oil
Department Reference: E3034-TDS-01-2019
 Acknowledgement

We would like to express our gratitude to all those who provided support in
this project for us. First is Associate Professor Taweedej Sirithanapipat, Ph.D., who is
our good teacher and our project advisor. He taught us how to think to design our
concept idea. He also gave us so many useful advices both related and unrelated to
us and this project. Even more he also provides facility for us. Thank you for all the
supports we really appreciated your kindness that you gave to us from the very
beginning. Second is Ajarn Varodom Toochinda, Ph.D., who is our project committee,
he gave us useful advice that made us saw the weak point directly. Third is Work Shop
Teachers at RDIPT that give us the advice and machining our machine very perfectly.
Fourth are our parents that support us the budget. Fifth is Lab, PID (Practical Intelligent
Design) that provide us facility and tools. Our project could not be complete without
their kind and great help. We truly appreciated everyone’s effort and commitment to
our success.

Ritthikiat Churoop 5810545327

Phanuwat Chaichutchouwakul 5910546163

ii
 Table of Contents
List of Figures................................................................................................................................. iii
Chapter 1. Introduction ............................................................................................................... 1
1.1 Background.......................................................................................................................1
1.2 Objective...........................................................................................................................2
1.3 Scope.................................................................................................................................2
1.4 Schedule...........................................................................................................................2
Chapter 2. Literature Review ...................................................................................................... 3
2.1 Essential oil ......................................................................................................................3
2.2 Type of Extraction ..........................................................................................................5
2.3 Thermodynamic phase diagram ............................................................................... 15
2.4 Properties of solvents affecting extracts ................................................................. 19
2.5 Raw material used in study ....................................................................................... 25
2.6 Pressure Vessel Design................................................................................................ 29
2.7 Material & Tools ........................................................................................................... 34
Chapter 3 Methodology ............................................................................................................ 48
3.1 Procedure ...................................................................................................................... 48
3.2 Material & Equipment ................................................................................................. 51
Chapter 4. Result ........................................................................................................................ 53
4.1 Designing Model ........................................................................................................... 53
4.2 Actual Model ................................................................................................................ 55
4.3 Control Unit (Thermostat ON/OFF) .......................................................................... 57
4.4 Result of Experiment................................................................................................... 57
4.5 Result & Discussion...................................................................................................... 60

i
Chapter 5 Conclusion ................................................................................................................ 61
5.1 Summary........................................................................................................................ 61
5.2 Future Work .................................................................................................................. 61
5.3 Recommendation ........................................................................................................ 63
Reference ..................................................................................................................................... 64
Appendices .................................................................................................................................. 66
Student Biographies ................................................................................................................... 94

ii
 List of Figures
Figure 1. Basic oil extraction methods ..................................................................................... 4
Figure 2. List of selected bioactive compounds with high nutraceutical potential. ...... 4
Figure 3. Cold-press extraction process ................................................................................... 6
Figure 4 .(A) Schema of an open-focused microwave-assisted extraction system. (B)
Schema of a closed vessel microwave-assisted extraction system. .................................. 7
Figure 5 .Representation of the two heating modes and temperature gradient: (a) by
convection and (b) by microwave energy ............................................................................... 7
Figure 6. Generalized Flowsheet of the Different Types of Steam Distillation ................ 8
Figure 7. Solvent extraction process......................................................................................... 9
Figure 8. Typical PLE configuration. Basic steps of PLE ...................................................... 10
Figure 9. Apparatus for pressurized-liquid extraction.......................................................... 10
Figure 10. Conventional Soxhlet extractor. ........................................................................... 11
Figure 11. Flow diagram of supercritical fluid extraction system ..................................... 12
Figure 12. The supercritical fluid extraction unit.................................................................. 13
Figure 13. Supercritical CO2 Extraction for Industry ............................................................ 13
Figure 14. Comparison of Extraction Techniques Used for Solid Samples ..................... 14
Figure 15. General Phase diagram ........................................................................................... 16
Figure 16. Phase diagram of CO2 with supercritical point .................................................. 18
Figure 17. Stress distribution in thick-walled cylinder subjected to internal pressure.
(a) Thick-walled cylinder (b) Tangential stress distribution (c) Radial stress distribution
........................................................................................................................................................ 29
Figure 18. Design of thick-walled cylinder with a wall thickness of 6 mm .................... 30
Figure 19. The one-eight segment of the cylinder with a wall thickness of 6 mm. ..... 30
Figure 20. The boundary conditions of the finite element method using ANSYS ........ 31
Figure 21. Show the input parameter of the vessel............................................................ 31
Figure 22. Mechanical properties of materials...................................................................... 32

iii
Figure 23. Hoop and longitudinal stress of cylinder with wall thickness difference (a) 6
mm, (b) 7 mm, (c) 8 mm........................................................................................................... 32
Figure 24. Comparison between analytic and simulation of the maximum hoop and
longitudinal stress with wall thickness and internal pressure variations ........................ 33
Figure 25. Carbon seamless steel pipe .................................................................................. 34
Figure 26. Blind flange SC forty-five ........................................................................................ 35
Figure 27. Stud or Threaded rod ............................................................................................. 36
Figure 28. O - Ring....................................................................................................................... 37
Figure 29. O - Ring used in experiment .................................................................................. 37
Figure 30. Pressure gauge with cross section ........................................................................ 38
Figure 31. Microcontroller (Arduino) ....................................................................................... 39
Figure 32. Thermocouple Type K ............................................................................................ 40
Figure 33. Fiberglass Tape Heater ........................................................................................... 44
Figure 34. Needle valve and cross section............................................................................ 45
Figure 35. Voltage relay ............................................................................................................. 46
Figure 36. TM1637Display ......................................................................................................... 47
Figure 37. The process of CO2 Extraction by using 3 vessels ............................................ 49
Figure 38. The process of CO2 Extraction non-recirculated CO2 ....................................... 50
Figure 39. Solid work software ................................................................................................. 51
Figure 40. Temperature Control Unit (Schematic) ............................................................... 52
Figure 41. Design Model ............................................................................................................ 53
Figure 42. CAD Model ............................................................................................................... 54
Figure 43. Stand holder (360 degree rotate) ......................................................................... 55
Figure 44. Extraction Vessel ...................................................................................................... 55
Figure 45. Extraction vessel on stand holder........................................................................ 56
Figure 46. Extraction vessel that contain CO2 and specimens (inside) ............................ 56
Figure 47. Actual Control Unit on board................................................................................ 57
Figure 48. Pressure and Temperature reach the critical point after operate for 20
minutes. ........................................................................................................................................ 57
iv
Figure 49. Show temperature and pressure when the prototype operated.................. 58
Figure 50. Pressure increases with time ................................................................................. 58
Figure 51. Temperature increases with time......................................................................... 59
Figure 52. Oil remain on the valve’s surface ........................................................................ 59
Figure 53. Oil stains on the container (left) and remain inside the vessel (right) ......... 60
Figure 54. Leak around assuagement value screw .............................................................. 62

v
 Chapter 1. Introduction

1.1 Background

There are several ways to extract plant in natural by utilizing variety method
and many machines. Depend on method and the quality of essential oil, such as
“Steam Distillation” or “Solvent Extraction”. In which paramount substances are in
the form of essential oil. This gives little of terpene in plants compared to weight. This
caused constraint of extraction. In now a day there are a plethora of essential oils
demand in Pharmaceutical and Victuals industrial such as caffeine in coffee bean,
Xanthomas in mangos teen, Damascena in rose and limonene in bergamot leaf. These
substances need to import from abroad.
Due to the extraction of these substances, high technology is required and
invested entirely. The development of machines for extracting and studying the quality
of engenderment processes is ergo very compulsory. The exordium of solvent
extraction technology utilizing supercritical carbon dioxide as a solvent. The advantage
is a solvent that does not smell and taste that will perturb the extracted essential oils,
safe when utilized with pharmaceutical and aliment products, non-flammable
substance, low viscosity and easy to infiltrate. From the properties of carbon dioxide
at the critical point, they have the same liquid and gas characteristics. It's facile to
adjust the pressure, which will make the state of carbon dioxide into gas. There is no
solvent left in the product. The extraction condition can be adjusted by pressure and
temperature felicitous for extraction of sundry plants, but these machines are huge
using mass product causing high cost and unmovable. This project is focusing on
designing mobile extraction machine for portable, decreasing process duration and
cost.

1
1.2 Objective

- Design and Prototype of The Carbon Dioxide Super Critical Fluid

Extraction.

1.3 Scope

- Able to create a real prototype and operate the condition of supercritical

CO2 extraction.
- Easy to move as a portable device and reduce cost for localization.

1.4 Schedule

Time OCT NOV FEB MAR APR MAY JUN

Activities 2019 2019 2020 2020 2020 2020 2020

Discuss the scope of

project with consultant

Study extraction type

Design model sketch

Make CO2 Extraction

Prototype

Collect and analysis

the data

Write report

Presentation

2
 Chapter 2. Literature Review

2.1 Essential oil

Essential oils are natural products, derived from aromatic plants, traditionally
used all over the world for disinfection, as anti-inflammatory, relaxing, and stimulating
substances, and with potential and modern exploitation in clinical medicine. The
earliest recorded mention of the techniques and methods used to produce essential
oils is believed to be that of Ibn al-Baitar (1188 – 1248). The chemical composition of
these essential oils varies widely depending upon the geographical location, botanical
origin, genetics, bacterial endophytes, and extraction techniques. Essential oils are
commonly used in food and cosmetic industries. They can be used as natural
alternatives to synthetic preparations to prevent and treat infectious diseases. They
are used traditionally to treat other diseases like respiratory tract, digestive system,
gynecological, andrological, endocrine, cardiovascular, nervous system, and skin
infections [1].
2.1.1 Use of Essential Oils
The use of essential oils is extremely diverse depending on the source,
quality, extraction procedure, etc. Essential oils have proven industrial applications in
the manufacture of perfumes, cosmetics, soap, shampoos, or cleaning gels. Another
interesting aspect of these oils is their potential as therapeutic agents in aromatherapy
or as active principles or excipients of medicines. Another significant application of
essential oils is in the agri-food industry, both for producing beverages and for flavoring
foods.
2.1.2 Oil Extraction
Oil extraction is defined as the process of separating triglyceride (TAG) lipids
from the harvested and concentrated algal biomass and it could be done through a
variety of mechanical or chemical manipulation techniques as shown in Figure 1.

3
 Figure 1. Basic oil extraction methods
2.1.2 Commercial plants
The market for natural resource-based products is steadily increasing, with
essentially around-the-clock screening of plants in the hope of discovering new natural
compounds that could prove to be of value in the food, cosmetics, and
pharmaceutical sectors for development of a variety of products. These seven different
plant species (Figure 2) are found in different parts of the world and they represent a
rich source of bioactive components [2].

Figure 2. List of selected bioactive compounds with high nutraceutical potential.

4
2.2 Type of Extraction

Essential oils are the liquids that are isolated from plants when introduced to
solvents, they are liquefied versions of the plants. Popular extraction methods include
Steam Distillation, Solvent Extraction, CO2 Extraction, Maceration, Enfleurage, Cold
Press Extraction, and Water Distillation. The method of extraction affects essential oil
quality by way of pressure and temperatures applied.

Some extraction methods are best suited to particular plant types and parts
for example, Cold Press extraction is better than Enfleurage for obtaining oils from
citrus fruit peels, because the peels need to be pierced and squeezed, which is not
achievable through Enfleurage.

2.2.1 Mechanical Extraction (MAE)

- Cold-Press Extraction
Cold press extraction is one of the methods of mechanical extraction
as well as required less energy than other oil extraction techniques and also
environmentally friendly. It is used to extract oil from a range of matrices and is
produced especially in the oil production from oilseeds. High – quality oils can be
obtained by performing production at low temperatures using cold press method. It
has an environmentally friendly use with no solvents. In other words, the cold-press
extraction does not involve either heat or chemical extraction. The soybean, sunflower,
rapeseed, corn, grapeseed, hemp, flaxseed, rice bran, olive and pumpkin oils were
obtained by cold press extraction method. Moreover, these oils are interesting for
consumers due to their natural and safe as well as prevent certain diseases and
improve human health due to including a higher level of lipophilic phytochemicals
such as antioxidants. These oils have better nutritive properties than refined oils.
However, they have a lot of advantages, one of the disadvantages of this technique is
low productivity. Another disadvantage of this technique is hard to extract same quality
product. The cold pressed oils can add to food as natural antioxidative additives due
to phytochemicals and as fatty acid supplements due to invaluable double bond fatty

5
acid. There are several studies to investigate the other chemical compounds in the oils
and try to use in food products [3].

Figure 3. Cold-press extraction process

- Microwave-Assisted Extraction (MAE)

Microwave-assisted extraction (MAE) uses microwave energy in sample
treatment. It depends on the dielectric susceptibility of both the solvent used and the
matrix. Microwave energy causes molecular turbulence by ion migration and dipole
rotation. Unlike classical conductive heating methods, microwaves heat the whole
sample simultaneously without heating the vessel. Moreover, as microwave radiations
are focused directly on the sample, heating is more efficient and thus homogeneity
and reproducibility greatly improve. Therefore, the boiling point of the solution is
reached very quickly, leading to short extraction times. The application of microwave
energy to the samples may be performed using two techniques: open vessels at
atmospheric pressure, or closed vessels under controlled pressure and temperature.
Both systems are schematized in (Figure 4). Automation is possible and the
commercially available apparatus allows a simultaneous extraction of 24 samples. The
principal interest resides in the possibility to adjust extraction selectivity by choosing
the solvent [4].

6
Figure 4 .(A) Schema of an open-focused microwave-assisted extraction system. (B)
Schema of a closed vessel microwave-assisted extraction system.

Figure 5 .Representation of the two heating modes and temperature gradient: (a) by
convection and (b) by microwave energy

7
 2.2.2 Chemical Extraction

- Steam distillation
Steam distillation is a process used for the recovery of volatile
compounds with high boiling point, from inert and complex matrices, solid or liquid,
using saturated or superheated steam as separation and energy agent (Cerpa et al.,
2008). This process is used for the extraction of essential oil from plants (Palma et al.,
2013). In practice, the process uses water and/or steam as extracting agent to vaporize
or liberate the volatile compounds from the raw material. The compounds are
volatilized by absorbing heat from the steam, and are then transported to the steam
where they are diffused. The resulting vapor phase is cooled and condensed prior to
separating the water from the organic phase based on their immiscibility. In this
process, two products are obtained: volatile oil and hydrosol. The volatile oil is in the
upper phase and the hydrosol (water and some hydrolyzed compounds) is in the
bottom phase of the decanter. According to the type of contact between the matrix
and the water and/or steam, there are three variants of the steam distillation process
(Figure 6) dry steam distillation (a), direct steam distillation (b), and hydro distillation
(water distillation) (c) [5].

Figure 6. Generalized Flowsheet of the Different Types of Steam Distillation

8
 - Solvent Distillation

This method employs food grade solvents like hexane and ethanol to
isolate essential oils from plant material. It is best suited for plant materials that yield
low amounts of essential oil, that are largely resinous, or that are delicate aromatics
unable to withstand the pressure and distress of steam distillation. This method also
produces a finer fragrance than any type of distillation method. Through this process,
the non-volatile plant material such as waxes and pigments, are also extracted and
sometimes removed through other processes.

Once the plant material has been treated with the solvent, it produces
a waxy aromatic compound called a “concrete.” When this concrete substance is
mixed with alcohol, the oil particles are released. The aforementioned chemicals used
in the process then remain in the oil and the oil is used in perfumes by the perfume
industry or for aromatherapy purposes [6].

Figure 7. Solvent extraction process

- Pressurized liquid extraction (PLE)
Pressurized liquid extraction (PLE), also known as accelerated solvent
extraction (ASE), is an extraction technique that operates under high temperature and
pressure. The extractants are maintained in a liquid state (subcritical) even at a
temperature higher than boiling point if high pressure is applied. The elevated
temperature can dramatically increase the solubility and diffusion of analytes resulting
in less extraction time and lower solvent consumption. PLE is becoming increasingly

9
popular in natural products extraction due to these advantages. A wide range of
carotenoids with different polarities were extracted within 5 minutes under 103 Bar
using PLE from three types of fruits, Tunisian kaki, peach, and apricot. The property of
natural products extracted is also influenced by the pressure used in PLE. Xi et al.
compared the recovery and antioxidant activities of total phenolic compounds
extracted from green tea under pressures ranging from 150 to 450 MPa. The extracted
phenolic compounds not only exhibited higher yields under 450 MPa but also stronger
antioxidant activities [7].

Figure 8. Typical PLE configuration. Basic steps of PLE

Figure 9. Apparatus for pressurized-liquid extraction.

10
 - Soxhlet extraction
Soxhlet extraction is only required where the desired compound has a
limited solubility in a solvent, and the impurity is insoluble in that solvent. If the
desired compound has a high solubility in a solvent then a simple filtration can be
used to separate the compound from the insoluble substance. The advantage of this
system is that instead of many portions of warm solvent being passed through the
sample, just one batch of solvent is recycled. This method cannot be used for
thermolabile compounds as prolonged heating may lead to degradation of
compounds (Sutar et al., 2010).

Figure 10. Conventional Soxhlet extractor.

The experimental Soxhlet extraction apparatus consists of a distillation
flask, sample holder (thimble), siphon and condenser. A Soxhlet extraction procedure
usually involves the following steps. First, the sample material is packed in filter paper
and placed in the thimble. Next, vapors of a fresh solvent, produced in a distillation
flask, pass through the thimble containing the material to be extracted and are
liquefied in the condenser. When the liquid reaches the overflow level in the thimble,
a siphon aspirates the solution, and the liquid falls back into the distillation flask,
carrying the extracted solutes into the bulk liquid. The separation of solute from
solvent takes place in the distillation flask. Then solute is left in the flask and fresh

11
solvent vapors pass back into the solid bed of sample material. The operation is
repeated until complete extraction is achieved [8].

- Supercritical Fluid Extraction (SFE)

The supercritical extraction method is a new separation technique
developed in recent years. It is used to extract and separate substances using a
supercritical fluid as a solvent. Both the temperature and pressure of the supercritical
fluid are higher than the critical point. The supercritical fluid has similar density to an
ordinary fluid and many substances have a good solubility in it. Meanwhile, it also
keeps the transfer properties and easy penetration characteristics of gas. Small changes
in temperature or pressure near the critical point will cause a very significant change
in the density of the supercritical fluid. With this characteristic, it is easy to separate
solvent and extract. In recent years, the supercritical extraction method has been
widely used in the food, chemical, pharmaceutical, and environmental fields (Lv et al.,
2000). Supercritical CO2 is the most commonly used extraction solvent in the fine
chemical industry, especially in the extraction of fragrance, food additives, and
surfactants. Many studies have shown that supercritical CO2 is very effective in the
removal of oil, but phospholipid classification is still in the research stage mainly
because phospholipids are not soluble in supercritical CO2 [9].

Figure 11. Flow diagram of supercritical fluid extraction system

12
 - Supercritical CO2 extraction
Supercritical carbon dioxide has been identified as one of the
alternatives to water-based conventional processes. A supercritical fluid actually has
physical properties somewhere between those of a liquid and a gas. Supercritical fluids
are able to spread out along a surface more easily than a true liquid because they
have lower surface tensions than liquids. At the same time, a supercritical fluid
maintains a liquid’s ability to dissolve substances that are soluble in the compound,
which a gas cannot do. Supercritical fluids are by definition at a temperature and
pressure greater than or equal to the critical temperature and pressure of the fluid.
The critical pressure of CO2 is about 73.7 Bar and the critical temperature is about 31°C,
so supercritical applications using CO2 typically operate at temperatures between 32
and 49°C and pressures between 73.7 Bar and 241.3 Bar. A pressure-temperature (P-T)
phase diagram, shown in (Figure 16) (Anon, 2011) [10].

Figure 12. The supercritical fluid extraction unit

Figure 13. Supercritical CO2 Extraction for Industry

13
 - Comparison of extraction methods
There are several methods for extracting plant material, each method
will give different results. Some methods will provide essential oils which come from
Distillation and Expression only. Other methods will get Aromatic Extracts, which is not
considered as essential oils. From the following table, comparing the advantages and
disadvantages of each method of extraction [11].

Figure 14. Comparison of Extraction Techniques Used for Solid Samples

- Advantages of the supercritical CO2 extraction
In the supercritical CO2 extraction method, supercritical CO2 is used as
a solvent to remove oils and other nonpolar and weakly polar impurities in the
material to obtain high purity phospholipids. The operating pressure is up to
approximately 30 MPa and the operating temperature is only 40 – 60°C, which will not
cause deterioration of phospholipids by heating. Because supercritical fluid has very
good mass transfer performance, the extraction time is short and CO2 escapes in a
gaseous state after relief, without solvent residue. The insoluble content of acetone
can reach 98% by one operation. This method features easy operation, low production
costs, and good product quality but requires high investment in equipment. Compared
with other organic solvents, phospholipid extraction with supercritical CO2 has higher
purity and there is no toxic and hazardous organic solvent residue in the product. As
14
the extraction process proceeds in a mild condition at room temperature and without
oxygen, oxidation of phospholipids is greatly reduced [9].

2.3 Thermodynamic phase diagram

Phase diagram is a graphical representation of the physical states of a substance

under different conditions of temperature and pressure. A typical phase diagram has
pressure on the y-axis and temperature on the x – axis. As we cross the lines or curves
on the phase diagram, a phase change occurs. In addition, two states of the substance
coexist in equilibrium on the lines or curves. A phase transition is the transition from
one state of matter to another. There are three states of matter liquid, solid, and gas.
- Liquid: A state of matter that consists of loose, free moving particles which
form the shape set by the boundaries of the container in which the liquid is in. This
happens because the motion of the individual particles within a liquid is much less
restricted than in a solid. One may notice that some liquids flow readily whereas some
liquids flow slowly. A liquid’s relative resistance to flow is viscosity.
- Solid: A state of matter with tightly packed particles which do not change the
shape or volume of the container that it is in. However, this does not mean that the
volume of a solid is a constant. Solids can expand and contract when temperatures
change. This is why when you look up the density of a solid, it will indicate the
temperature at which the value for density is listed. Solids have strong intermolecular
forces that keep particles in close proximity to one another. Another interesting thing
to think about is that all true solids have crystalline structures. This means that their
particles are arranged in a three-dimensional, orderly pattern. Solids will undergo phase
changes when they come across energy changes.
- Gas: A state of matter where particles are spread out with no definite shape
or volume. The particles of a gas will take the shape and fill the volume of the
container that it is placed in. In a gas, there are no intermolecular forces holding the

15
particles of a gas together since each particle travels at its own speed in its own
direction. The particles of a gas are often separated by great distances.
Phase diagrams illustrate the variations between the states of matter of
elements or compounds as they relate to pressure and temperatures. The following is
an example of a phase diagram for a generic single-component system.

Figure 15. General Phase diagram

- Triple point – the point on a phase diagram at which the three states of
matter: gas, liquid, and solid coexist.
- Critical point – the point on a phase diagram at which the substance is
indistinguishable between liquid and gaseous states.
- Fusion(melting) (or freezing) curve – the curve on a phase diagram which
represents the transition between liquid and solid states.
- Vaporization (or condensation) curve – the curve on a phase diagram which
represents the transition between gaseous and liquid states.
- Sublimation (or deposition) curve – the curve on a phase diagram which
represents the transition between gaseous and solid states.

16
 Phase diagrams plot pressure (typically in atmospheres) versus temperature
(typically in degrees Celsius or Kelvin). The labels on the graph represent the stable
states of a system in equilibrium. The lines represent the combinations of pressures
and temperatures at which two phases can exist in equilibrium. In other words, these
lines define phase change points. The red line divides the solid and gas phases,
represents sublimation (solid to gas) and deposition (gas to solid). The green line
divides the solid and liquid phases and represents melting (solid to liquid) and freezing
(liquid to solid). The blue divides the liquid and gas phases, represents vaporization
(liquid to gas) and condensation (gas to liquid). There are also two important points on
the diagram, the triple point and the critical point. The triple point represents the
combination of pressure and temperature that facilitates all phases of matter at
equilibrium. The critical point terminates the liquid/gas phase line and relates to the
critical pressure, the pressure above which a supercritical fluid form.
With most substances, the temperature and pressure related to the triple point
lie below standard temperature and pressure and the pressure for the critical point
lies above standard pressure. Therefore, at standard pressure as temperature increases,
most substances change from solid to liquid to gas, and at standard temperature as
pressure increases, most substances change from gas to liquid to solid [12].
- CO2 Phase Diagram
The Supercritical CO2 extraction process creates phase changes in
carbon dioxide utilizing temperature and pressure. CO2 is known as a “tunable solvent”
making it extremely versatile for creating a multitude of end products by controlling
temperature and pressure. These phase One of the most amazing things about
extracting with CO2 is the ability to separate individual compounds as the extraction is
taking place. This also requires a system that will allow for stable temperature and
pressure changes during a single run changes create an environment to drop out
differing weights of components in the plant material. Carbon dioxide (CO2) is the most
used supercritical fluid, sometimes modified by co-solvents such as ethanol or
methanol. Extraction conditions for supercritical carbon dioxide are above the critical
temperature of 31 °C and critical pressure of 73 Bar.

17
 Figure 16. Phase diagram of CO2 with supercritical point
Table1: Critical conditions for various solvents.
Critical conditions for various solvents
Molecular Critical Critical Critical
Solvent Mass Temperature Pressure Density
g/mol K MPa (atm) g/cm3
Carbon dioxide (CO2) 44.01 304.1 7.38 (72.8) 0.469
Water (H2O) 18.015 647.096 22.064 0.322
(217.755)
Methane (CH4) 16.04 190.4 4.60 (45.4) 0.162
Ethane (C2H6) 30.07 305.3 4.87 (48.1) 0.203
Propane (C3H8) 44.09 369.8 4.25 (41.9) 0.217
Ethylene (C2H4) 28.05 282.4 5.04 (49.7) 0.215
Propylene (C3H6) 42.08 364.9 4.60 (45.4) 0.232
Methanol (CH3OH) 32.04 512.6 8.09 (79.8) 0.272
Ethanol (C2H5OH) 46.07 513.9 6.14 (60.6) 0.276
Acetone (C3H6O) 58.08 508.1 4.70 (46.4) 0.278
Nitrous oxide (N2O) 44.013 306.57 7.35 (72.5) 0.452
Ammonia (polar) 132.5 11.28 0.240
Benzene(nonpolar) 289.0 4.89

18
 Carbon dioxide used in the experiment must concern about safety and clean.
Choosing Carbon dioxide should use food grade CO2 99.8%. From the following table
show the density of CO2 that use for extraction [13].

Table2: Solid CO2 and liquid CO2 with different density and purity.
Product Density
Beverage CO2 99.9%
Food grade CO2 99.8%
Liquid CO2 – USP > 99.5%
CO2 and Air 0.5 ppm – 50%
CO2 and Air 0.5 ppm – 50%
CO2 and He 0.5 ppm – 50%
CO2 and H2 0.5 ppm – 50%
CO2 and NO2 0.5 ppm – 50%

2.4 Properties of solvents affecting extracts

- Polarity
A solvent is a liquid that serves as the medium for a reaction. It can
serve two major purposes;

- Non-participatory to dissolve the reactants. Polar solvents are best for

dissolving polar reactants (such as ions); nonpolar solvents are best for dissolving
nonpolar reactants (such as hydrocarbons).

- Participatory as a source of acid (proton), base (removing protons), or

as a nucleophile (donating a lone pair of electrons). The only class of solvents for
which this is something you generally need to worry about are polar protic solvents.

19
 - Boiling Point
The boiling of solvent under atmospheric pressure or vacuum will
affected on the profile of extraction product. Therefore, the changing of solvent from
Methanol to Ethanol (or isopropanol and butanol) at atmospheric pressure will change
the molecular weight of extraction product thus the high boiling point solvent will
extract more the high molecular weight compounds.
- Viscosity
The viscosity of the solvent determines the ability of the penetrate into
the plant material, so the viscosity of the solvent determines the extraction efficiency,
as it reduces the duration time of extraction between the solvent and the plant
material.
- Latent Heat of Evaporation
By using low latent heat solvent in evaporation process has advantage
that solvent can be separated from the extract by using less energy than high heat of
evaporation solvent [13].
Table3: Show the polarity of each substance.
Solvent Chemical Formula Boiling Pt. Polarity Density
Non-Polar Solvents
Benzene C6H6 80 °C 2.3 0.879 g/ml
Toluene C6H5-CH3 111 °C 2.4 0.867 g/ml
Diethyl ether CH3CH2-O-CH2-CH3 35 °C 4.3 0.713 g/ml
Colloform CHCl3 61 °C 4.8 1.498 g/ml
Ethyl acetate CH3-C(=O)-O-CH2-CH3 77 °C 6.0 0.894 g/ml
Methylene chloride CH2Cl2 40 °C 9.1 1.326 g/ml
Polar Aprotic Solvents
Acetone CH3-C(=O)-CH3 56 °C 21 0.786 g/ml
Acetonitrile CH3-C≡N 82 °C 37 0.786 g/ml
Dimethyl formamide H-C(=O)-N(CH3)2 153 °C 38 0.944 g/ml

20
 Solvent Chemical Formula Boiling Pt. Polarity Density
Polar Protic Solvents
Acetic acid CH3-C(=O)-OH 118 °C 6.2 1.049 g/ml
n-Butanol CH3-CH2-CH2-CH2-OH 118 °C 18 0.810 g/ml
Isopropanol CH3-CH(-OH)- CH3 82 °C 18 0.785 g/ml
n-Propanol CH3- CH2- CH2-OH 97 °C 20 0.803 g/ml
Ethanol CH3- CH2-OH 79 °C 24 0.789 g/ml
Methanol CH3OH 65 °C 33 0.791 g/ml
Formic acid H-C(=O)-OH 100 °C 58 1.21 g/ml
Water H-O-H 100 °C 80 0.998 g/ml

2.4.1 Factors affecting Supercritical fluid extraction

- Pressure and Temperature
There are many parameters use to describe the behavior of solvent in
supercritical fluid extraction.
1. Miscibility or threshold pressure, it is the pressure that separate the partition.
2. Solubility pressure is the greatest point that solute can be dissolved.
3. Range between miscibility pressure and solubility pressure
4. Physical property of solvent especially boiling point, in general the solute is
well dissolve when the temperature is higher than melting point.

For example, naphthalene is slightly soluble in carbon dioxide at

pressure 75 Bar but when increase the pressure to 90 Bar this substance can be
maximum soluble which called maximum solubility pressure. Pressure of fluid is the
main factor affecting efficiency of extraction, increasing of pressure will increase density
of fluid and also affecting better solubility. Temperature is affecting evaporation of
solvents when increase temperature the better evaporation. But in practical volatile
oil extraction may not always adhere to this principle.

21
 Extraction of (Elettaria cardamomum Maton) found that increasing of
pressure affecting better yield but increasing of temperature affecting decreasing of
yield. When analyses volume of volatile oil left in the seed such as β-pinene, cineole,
linalool, α-terpineol and terpinyl acetate resulting in the opposite way.
Extraction of lavender found that increasing of temperature and
pressure result better antioxidant and yield. Mesomo and team extracted (Zingiber
officinale Roscoe) from ginger with supercritical CO2 extraction found that increasing of
pressure resulting higher yield percentage while increasing temperature affects the
product positive and negative way. At pressure 25 MPa, when increases temperature
from 293.15 K to 333.15 K result increasing of yield but at pressure 10 MPa increase
temperature form 293.15 K to 333.15 K result decreasing of yield. When consider
volatile oil volume of each types (α-zingiberene, β-sesquiphellandrene, α–farnesene)
found that at temperature 293.15 K and pressure 25 MPa resulting volatile oil decrease
comparing to pressure at 10 MPa.
According to the previous, the adjustment of the pressure and
temperature of extraction is not in accordance with the principle stipulated above,
and this will require adjustments to determine the appropriate conditions for the
extraction of oil from each plant.
- Modifier
Modifier is the additive add in Supercritical CO 2 for specific substance
but what concerned is exceed of adding modifier will cause parameter change. From
the research of Rudyk and his team found that using ethanol or methanol as the
modifier can increase yield from supercritical extraction, in which ethanol can extract
17 to 38 carbon compounds, while methanol extract to press compounds that contain
7 to 9 carbon. From extracting (Lippia alba Mill). At pressure 35 MPa and temperature
40 °C when not using ethanol as modifier can get 1.92% of yield. When use ethanol
5% and 10% ad modifier yield increase to 2.14% and 3.19% respectively.

22
 - Extraction time
From the study of the effect of sage (Salvia officinalis L.) leaf oil
extraction time on volatile oil content Including α-pinene, 1,8-cineole, γ-cardinene
and manool when changing the duration from 20 minutes to 350 minutes, found that
when using longer time, the amount of α-pinene and 1,8-cineole tends to decrease
but on the contrary, increasing time duration can be able to remove more cardinene
and manool. Changes in extraction duration result in the amount of each type of
volatile substance changed, such as the study of the amount of active substance in
the sage oil, when extract with different periods will be given to different substances.
When the extraction time increase, amount of substance sesquiterpenes and
oxygenated sesquiterpenes increased while terpenes and oxygenated terpenes
decreased. When considering extracted substance at the certain time, it was found
that if extract for 100 minutes, the most extracted substance is oxygenated terpenes,
followed by sesquiterpenes, terpenes, and oxygenated sesquiterpenes, respectively.
But if extracted for 350 minutes, the substance extracted the most was sesquiterpenes
followed by oxygenated terpenes, oxygenated sesquiterpenes, and terpenes,
respectively.
- Flow rate
Ferreira and his team studied how flow rate change affecting to
percentage of yield. From extracting (Piper nigrum L.) found that decreasing of CO2
flow rate from 0.6876 g/min to 0.0725 g/min (constant pressure and temperature at
200 Bar and 40 °C) can increase amount of yield which is related to study of
Papamichail that extracted (Apium graveolens L.) that decrease flow rate of CO2 3 kg/h
to 1.1 kg/h also can increase percentage of yield.
- Particle size
According to the research of Papamichail and his team, reducing particle
size of (Piper nigrum L.) from 490 µm to 210 µm can increase extracted yield which is
related to study of Louli that reducing size of (Petroselinum sativum Hoffm) seed from
495µm to 293µm can increase yield as well. Larkeche and his team (2015) extracted

23
essential oil from (Juniperus Communis L.) by supercritical CO2 extraction compared
with particle of herb has diameter 0.5 mm and less than 0.315 mm. From the
experiment found that using smaller size of herb can extract more essential oil
obviously but there is some study found that only an appropriate range of particle size
that will obtain big amount of extracts such as when the particle size of Cleome
coluteodes Boiss. Increased, yield increased as well but increase particle size further,
yield decreased [14].

2.4.2 The properties of supercritical carbon dioxide affect to the better

yield than another conventional extraction.
- Transportation Property
Supercritical carbon dioxide has low viscosity but high diffusion
coefficient that cause make it spread evenly and penetrate into solid structure or the
particle that have a good solvent. Diffusion coefficient depends on various factor such
as temperature, pressure therefore, temperature and pressure must be adjusted to the
appropriate point in order to get the best yield. Transpiration rate is the direct result
to viscosity and diffusion coefficient, also depends on diffusion distance.

- Solvent Power Property

Solubility of solvent is an outstanding property of supercritical CO2
which is higher than general liquid because parameter can be adjusted as you want,
by adjusting temperature in case of solvent is liquid. Increasing the temperature will
cause solubility of solvents increased. For supercritical CO2, increasing the temperature
will increase solubility of solvents as well. But at the same time increasing the
temperature will cause the density of supercritical CO2 decreased which will result
supercritical CO2 and solvent be apart resulting in decreasing solubility of the solvent.
This problem can be solved by adding pressure to supercritical CO2 to increase the
density until close to initial conditions. Therefore, keeping temperature and pressure
in the right condition can improve the properties of supercritical CO2 to be better suited
for extraction.

24
 - Selectivity Property
Selectivity property is another advantage of supercritical CO2 extraction
because supercritical CO2 can adjust temperature and pressure to have the appropriate
solubility for desired substance in extraction with the least contaminate unwanted
substances. For example, extracting natural products, if use supercritical CO2 extraction
instead of steam distillation and select only essential oils must use the solvent that
has a slow diffusion property, then adjust it into critical point but still in the suited
pressure range such as pressure 60 Bar, temperature 60 °C [13].

2.5 Raw material used in study

2.5.1 Coffee
Coffee is a brewed drink prepared from roasted coffee beans, the seeds of
berries from certain Coffea species. Once ripe, coffee berries are picked, processed,
and dried. Dried coffee seeds (referred to as "beans") are roasted to varying degrees,
depending on the desired flavor. Roasted beans are ground and then brewed with
near-boiling water to produce the beverage known as coffee.
Coffea is a genus of flowering plants in the family Rubiaceae. Coffea species
are shrubs or small trees native to tropical and southern Africa and tropical Asia. The
seeds of some species, called coffee beans, are used to flavor various beverages and
products. The fruits, like the seeds, contain a large amount of caffeine, and have a
distinct sweet taste and are often juiced.
Coffee is darkly colored, bitter, slightly acidic and has a stimulating effect in
humans, primarily due to its caffeine content. It is one of the most popular drinks in
the world, and it can be prepared and presented in a variety of ways (e.g., espresso,
French press, caffè latte).

25
 - Caffeine
Caffeine is a natural substance found in more than 60 plant species.
These include tea leaves, coffee beans, guarana and cocoa seeds. Caffeine can also
be produced synthetically and added to certain foods, beverages and medications.
Caffeine is one of a group of drugs called methylxanthines, which have several effects
on the body. They stimulate the central nervous system and increase the frequency
of urination (are diuretics), smooth muscle relaxation, which affects body systems
regulated by smooth muscles, including the endothelial system which regulates blood
flow.
- Decaffeination
Decaffeination is the removal of caffeine from coffee beans, cocoa, tea
leaves, and other caffeine-containing materials. Decaffeinated drinks contain typically
1–2% of the original caffeine content, and sometimes as much as 20%. Decaffeinated
products are commonly termed decaf.
In the case of coffee, various methods can be used for decaffeination.
These methods take place prior to roasting and may use organic solvents such as
methylene dichloride or ethyl acetate, supercritical CO2, or water to extract caffeine
from the beans while leaving flavor precursors in as close to their original state as
possible.
- Extraction by Supercritical CO2 process
In this process, green coffee beans are steamed and then added to a
high-pressure vessel. A mixture of water and liquid CO2 is circulated through the vessel
at 300 atm and 65 ºC (150°F). Caffeine dissolves into the CO2 compounds contributing
to the flavor of the brewed coffee are largely insoluble in CO2 and remain in the bean.
In a separate vessel, caffeine is scrubbed from the CO2 with additional water. The CO2
is then recirculated to the pressure vessel.

26
 2.5.2 Bergamot
Bergamot is one of several fragrant herbs of the genus Monarda (family
Lamiaceae) or the fruit of the bergamot orange (Citrus ×aurantium). The bergamot
herbs and the bergamot orange have a similar characteristic floral fragrance and are
commonly used in perfumes and as a flavoring. The bergamot orange is a citrus fruit
cultivated chiefly in Italy and is well known for its use in Earl Grey tea. The tree yields
a yellow-green pear-shaped fruit, the peel of which is valued by the flavoring and
perfume industries for its essential oil.
Bergamot essential oil is one of the main basic constituents for the manufacture
of perfumes, due to its ability to fix the aromatic bouquet of aromas and harmonize
all of the essences, enhancing the fragrance. BEO is also used by the pharmaceutical
industry, both to absorb the unpleasant smells of medicinal products and for its
antiseptic and antibacterial properties. Finally, BEO is used in the food and
confectionery industries as a flavoring.
In Italian folk medicine, it has been used primarily for fever and parasitic
diseases, in addition to mouth, skin, respiratory and urinary tract infections, gonococcal
infections, leucorrhoea, vaginal pruritus, tonsillitis, and sore throats (Pendino, 1998).
For its antiseptic and antibacterial proprieties, BEO has been used as an antimicrobial
agent to facilitate wound healing and has been included in preparations used to treat
upper respiratory-tract disorders and hyperhidrosis.
- Extraction by Supercritical CO2 process
In this process, bergamot leaf is steamed and then added to a high-
pressure vessel. A mixture of water and liquid CO2 is circulated through the vessel at
80 Bar and 50 ºC. limonene dissolves into the CO2; compounds contributing to the
terpene of the bergamot are largely insoluble in CO2 and remain in the leaf. In a
separate vessel, limonene is scrubbed from the CO2 with additional water. The CO2 is
then recirculated to the pressure vessel.

27
 2.5.3 Mangosteen Peel
Mangosteen is associate actual fruit that has been around for thousands of
years, notwithstanding you haven’t detected of it. Mangosteen is usually mature in
geographic region, however due to its various health edges, has become a quick
growing import to different countries. The fruit itself wants terribly tropical (hot, humid,
and wet) conditions to grow; thus, makes an attempt to grow mangos teen fruit in
different areas are unsuccessful. The fruit is especially mature in China, Singapore,
Taiwan, Indonesia, Malaysia, Cambodia, and also the Philippines. This is often as a
result of it wants the climate of those areas to thrive.
Mangosteen fruit grows on a tree, however not simply a standard tree.
Mangosteen trees grow in deep wealthy soils, and grow twenty to eighty feet tall. The
tree has thick evergreen leaves, and blooms reaching upwards of a foot in breadth.
The bark of the tree is sort of black. So, simply because the name mangosteen fruit
sounds kind of like the popular mango, they’re nothing alike. Fruits are harvested by
ladder or cutting pole. Mangosteen fruit is understood for its varied health edges. It’s
loaded with xanthones (promotes healthy body function), and a serving of mangos
teen fruit contains up to a humongous five grams of fiber. Overwhelming mangosteen
will boost the body’s system, increase physical attraction, and increase energy levels.
Mangosteen fruit has additionally been joined to promoting prostate health in men
and bone and joint health in girls. The mangosteen can even facilitate maintain enteral
health.
- Extraction by Supercritical CO2 process
In this process, Mangosteen peels are steamed and then added to a
high-pressure vessel. A mixture of water and liquid CO2 is circulated through the vessel
at 300 Bar and 60ºC (from the research). Xanthones dissolves into the CO2 compounds
contributing to the flavor of the mangosteen peels are largely insoluble in CO2 and
remain in the peels. In a separate vessel, the essential compounds are scrubbed from
the CO2 with additional water. The CO2 is then recirculated to the pressure vessel. The
supercritical fluid CO2 extracts the aromatics from the plant material.

28
2.6 Pressure Vessel Design

2.6.1 Thick-Walled Cylinder

Stress in thick-walled cylinder, the thin-walled and thick-walled are
classifications of pressure vessels based on their dimensions. The thin-walled pressure
vessel in which the wall thickness (t) is less than 1 / 20 of the internal diameter (d).
On the other hand, the thick-walled in which the wall thickness (t) is more significant
than 1 / 20 of it (d). The vessel in this study is assumed to be a thick-walled cylinder.
In the case of a thick-walled, as shown in (Figure 17) (a), stress on parts of the wall
cannot be assumed to be evenly distributed. The tangential and radial stresses
develop by considering values that depend on the radius of the element. Figure 17 (b)
and (c) show the stress distributions on thick-walled cylinders.

Figure 17. Stress distribution in thick-walled cylinder subjected to internal pressure.

(a) Thick-walled cylinder (b) Tangential stress distribution (c) Radial stress distribution

Theory of Elasticity is the primary theory for the thick-walled cylinder, which
produces a stress condition as a continuous function of the radius above the wall of
the pressure vessel. The stress in a cylindrical pressure vessel depends on the ratio of
the inner radius to the outer radius (𝑟0 / 𝑟𝑖 ) rather than cylinder size. The thick-walled
cylinder pressure will occur in three directions, namely hoop (circumferential or
tangential), longitudinal (axial), and radial. The maximum stress equations in thick-
walled cylinders in the hoop, longitudinal, and radial directions are;

29
 𝑟02 + 𝑟𝑖2
(𝜎𝑛 )𝑚𝑎𝑥 = 𝑝𝑖 ( 2 )
𝑟0 − 𝑟𝑖2
𝑟𝑖2
(𝜎𝑙 )𝑚𝑎𝑥 = 𝑝𝑖 ( 2 )
𝑟0 − 𝑟𝑖2
(𝜎𝑟 )𝑚𝑎𝑥 = −𝑝𝑖

where 𝑝𝑖 = internal pressure, 𝑟0= outer radius of cylinder, and 𝑟𝑖 = inner radius of
cylinder.

2.6.2 Finite Element Analysis

Figure 18. shows the model geometry of the cylinder. Since the geometry
exhibits asymmetry in the axial (Y), then it can model only the top half of it. The finite
element analysis used a 90-degree segment of the solid model of the cylinder. The
symmetric nature of the geometry and loading means that displacements are zero in
directions normal to the face exposed by the vertical and horizontal cuts employed
create this one-eight segment of the cylinder (Figure 19).

Figure 18. Design of thick-walled cylinder with a wall thickness of 6 mm

Figure 19. The one-eight segment of the cylinder with a wall thickness of 6 mm.
30
 The following assumptions are made theoretically on thick-walled cylinders.
I. Aluminum 6061 is homogeneous and isotropic. CFRP and GFRP are linearly elastic,
initially free of stress and defect. The fiber and matrix are homogenous, linearly elastic,
and isotropic. II. The cylinder section remains flat even after applying internal pressure.
III. All cylinder surface will expand or contract independently. The boundary conditions
of the finite element method using ANSYS software are shown in Figure 20 and input
parameters in Figure 21.

Figure 20. The boundary conditions of the finite element method using ANSYS

Figure 21. Show the input parameter of the vessel

The criteria for vessel material are lightweight and high strength. Aluminium
6061, Carbon Fiber Reinforced Polymer (CFRP), and Glass Fiber Reinforced Polymer
(GFRP) are chosen for it. The material properties of Aluminium 6061, CFRP, and GFRP
are shown in Figure 21. The data of mechanical properties of materials using Autodesk
Material Library.

31
 Figure 22. Mechanical properties of materials

Figure 23. shows the effect of wall thickness on the hoop and longitudinal
stress of the cylinder with an internal pressure of 2 MPa. The simulation results show
that the thicker the cylinder wall, the maximum hoop and longitudinal stress
decreases. The relationship between wall thickness and maximum hoop and
longitudinal stress is inversely proportional.

Figure 23. Hoop and longitudinal stress of cylinder with wall thickness difference (a)
6 mm, (b) 7 mm, (c) 8 mm.
Otherwise, if the internal pressure of the cylinder increases, then the
maximum hoop and longitudinal stress increases (Figure 24). The relationship between
internal pressure and maximum hoop and longitudinal stress is linear. Both values of
stress using finite element analysis are not significant difference using analytic - the
error percentage between finite element analysis and analytical less than 1 percent.
The hoop stress is always tensile, and maximum hoop stress always occurs at the inner
radius or the outer radius depending on the direction of the pressure gradient. If the
thick-walled cylinder subjected to external pressure only, then the maximum hoop

32
stress occurs at the outer radius (𝑟 = 𝑟0). In the research, the thick-walled cylinder
subjected to internal pressure only, then the maximum hoop stress occurs at the inner
radius (𝑟 = 𝑟𝑖 ). When the cylinder has closed ends the internal pressure acts on them
to develop a force along the axis of the cylinder. It is called the longitudinal stress and
is usually less than the hoop stress. In the research, the hoop stress higher than
longitudinal stress. The longitudinal stress values are about 41- 44 percent than the
hoop stress. Aluminum 6061, Carbon Fiber Reinforced Polymer (CFRP), and Glass Fiber
Reinforced Polymer (GFRP) can withstand maximum hoop and longitudinal stress. The
three materials have a tensile strength exceeding the two maximum stresses (hoop
and longitudinal). It means the materials can be used as rocket material case without
end caps [18].

Figure 24. Comparison between analytic and simulation of the maximum hoop and
longitudinal stress with wall thickness and internal pressure variations

33
2.7 Material & Tools

- Carbon seamless steel pipe (Standard API 5L GR. B / ASTM A106 GR. B
/ DIN1629 ST52.0)
Carbon seamless steel pipe is a plain carbon steel defined by its
mechanical properties again controlled Sulphur addition improves machinability due
to this experiment is not concerned about hygiene or eatable substance so we chose
steel AISI 1024 which is cheaper than stainless steel but has enough property that can
resist the pressure operate at 200 Bar – 300 Bar.

Figure 25. Carbon seamless steel pipe

Table 4. Carbon seamless steel pipe properties.

Ultimate Yield Elastic Fatigue Shear Shear Maximum
Tensile point Modulus Strength Strength Modulus Temperature
Strength (MPa) (GPa) (MPa) (MPa) (GPa) (°C)
(MPa)
785 590 190 230 360 73 400

Carbon seamless steel pipe has good machinability in a normalized or

hot-rolled condition. Based on the recommendations given by the machine
manufacturers, operations like tapping, milling, broaching, drilling, turning and sawing
can be carried out on suitable feeds, tool type, and speeds.

34
 - Blind flange (JIS 10K 3”)

Figure 26. Blind flange SC forty-five

A blind flange is a disc, collar or ring that attaches to pipe with the
purpose of providing increased support for strength, blocking off a pipeline or
implementing the attachment of more items. They are usually welded or screwed to
the pipe end and are connected with bolts. A gasket is inserted between the two
mating flanges to provide a tighter seal.
Blind flanges (Figure 30) are used to seal the end of a piping system or pressure
vessel openings to prevent flow. They are commonly used for pressure testing the
flow of liquid or gas through a pipe or vessel. They also allow easy access to the pipe
in the event that work must be done inside the line. Blind pipe flanges are often used
for high pressure applications.

35
 - Stud (Threaded rod)

Figure 27. Stud or Threaded rod

A type of metal fastener with threads that is cut into both the ends is
known as threaded rods. These rods almost resemble a screw but are longer and
thicker. The diameter is the same along the complete length. These rods sometimes
feature along the entire length and at times only at the either end. This depends upon
the model that is been used. They are at times referred to as all-thread or sometimes
simply stud. The threaded rod Fairfield is basically used to fasten wood or metal
together. It acts as a pin that is used to connect two materials together.
The threaded rod Fairfield is a versatile product that is used in all types
of industries such as, electrical, agricultural and construction. It is more popular as it
eliminates the need for raw material. You will also not require threading equipment or
any type of dies. These rods are produced with threads and is rolled under high
pressure. This gives them greater strength therefore can be used along with standard
nuts and washers.
The benefit with the rods is that they can be cut with the help of metal
cutting hack saw or may be power band saw. This makes the nuts move easily over
the threads. It is seen to be quite popular in plumbing and contractor fields. It is more
needed in places where cleanliness and attractiveness are necessary. It is greatly
resistant to corrosion so is widely used in medical, maintenance and machinery.

36
 - O - ring
An O - ring is a mechanical gasket in the shape of a torus; it is a loop of
elastomer with a round cross-section, designed to be seated in a groove and
compressed during assembly between two or more parts, creating a seal at the
interface.
O - rings are one of the most common seals used in machine design
because they are inexpensive, easy to make, reliable and have simple mounting
requirements. They have been tested to seal up to 5000 psi (35 MPa) of pressure. The
maximum recommended pressure of an O - ring seal depends on the seal hardness
and gland clearance.

Figure 28. O - Ring

Figure 29. O - Ring used in experiment

37
 - Pressure Gauge
Pressure gauge is an instrument for measuring the condition of a fluid
(liquid or gas) that is specified by the force that the fluid would exert, when at rest, on
a unit area, such as pounds per square inch or newtons per square centimeter.

Figure 30. Pressure gauge with cross section

The reading on a gauge, which is the difference between two pressures,

is known as the gauge pressure. If the lower of the pressures is the pressure of the
atmosphere, the total, or absolute, pressure is the sum of the gauge and atmospheric
pressures.
The Bourdon – tube gauge (Figure 34), invented about 1850, is still one
of the most widely used instruments for measuring the pressure of liquids and gases
of all kinds, including steam, water, and air up to pressures of 100,000 pounds per
square inch (70,000 newtons per square cm). The device (also shown in the figure)
consists of a flattened circular tube coiled into a circular arc. One end is soldered to a
central block and is open to the fluid whose pressure is to be measured; the other
end is sealed and coupled to the pointer spindle. When the pressure inside the tube
is greater than the outside pressure, the tube tends to straighten, thus turning the
pointer. The pressure is read on a circular scale.

38
 - Microcontroller (Arduino)
Arduino Uno is a microcontroller board based on the ATmega328P
(datasheet). It has 14 digital input / output pins (of which 6 can be used as PWM
outputs), 6 analog inputs, a 16 MHz ceramic resonator (CSTCE16M0V53-R0), a USB
connection, a power jack, an ICSP header and a reset button. It contains everything
needed to support the microcontroller simply connect it to a computer with a USB
cable or power it with an AC-to-DC adapter or battery to get started.

Figure 31. Microcontroller (Arduino)

You can tinker with your Uno without worrying too much about doing
something wrong, worst case scenario you can replace the chip for a few dollars and
start over again. "Uno" means one in Italian and was chosen to mark the release of
Arduino Software (IDE) 1.0. The Uno board and version 1.0 of Arduino Software (IDE)
were the reference versions of Arduino, now evolved to newer releases. The Uno board
is the first in a series of USB Arduino boards, and the reference model for the Arduino
platform for an extensive list of current, past or outdated boards see the Arduino index
of boards.

39
 - Thermocouple

Figure 32. Thermocouple Type K

A thermocouple is an electrical device consisting of two dissimilar electrical
conductors forming an electrical junction. A thermocouple produces a temperature-
dependent voltage as a result of the thermoelectric effect, and this voltage can be
interpreted to measure temperature. Thermocouples are a widely used type of
temperature sensor.
Commercial thermocouples are inexpensive, interchangeable, are supplied
with standard connectors, and can measure a wide range of temperatures. In contrast
to most other methods of temperature measurement, thermocouples are self-
powered and require no external form of excitation. The main limitation with
thermocouples is precision. system errors of less than one degree Celsius (°C) can be
difficult to achieve.
Thermocouples are widely used in science and industry. Applications include
temperature measurement for kilns, gas turbine exhaust, diesel engines, and other
industrial processes. Thermocouples are also used in homes, offices and businesses as
the temperature sensors in thermostats, and also as flame sensors in safety devices
for gas-powered appliances.
Certain combinations of alloys have become popular as industry standards.
Selection of the combination is driven by cost, availability, convenience, melting point,

40
chemical properties, stability, and output. Different types are best suited for different
applications. They are usually selected on the basis of the temperature range and
sensitivity needed. Thermocouples with low sensitivities (B, R, and S types) have
correspondingly lower resolutions. Other selection criteria include the chemical
inertness of the thermocouple material and whether it is magnetic or not. Standard
thermocouple types are listed below with the positive electrode (assuming Tsense >
Tref ) first, followed by the negative electrode.

Nickel-alloy thermocouples
Type E
Type E (chromel – constantan) has a high output (68 µV/°C), which makes it
well suited to cryogenic use. Additionally, it is non-magnetic. Wide range is −50 °C to
+740 °C and narrow range is −110 °C to +140 °C.
Type J
Type J (iron–constantan) has a more restricted range (−40 °C to +750 °C) than
type K but higher sensitivity of about 50 µV/°C. The Curie point of the iron (770 °C)
causes a smooth change in the characteristic, which determines the upper temperature
limit. Note, the European/German Type L is a variant of the type J, with a different
specification for the EMF output (reference DIN 43712:1985-01).
Type K
Type K (chromel – alumel) is the most common general-purpose thermocouple
with a sensitivity of approximately 41 µV/°C. It is inexpensive, and a wide variety of
probes are available in its −200 °C to +1350 °C (−330 °F to +2460 °F) range. Type K was
specified at a time when metallurgy was less advanced than it is today, and
consequently characteristics may vary considerably between samples. One of the
constituent metals, nickel, is magnetic, a characteristic of thermocouples made with
magnetic material is that they undergo a deviation in output when the material reaches
its Curie point, which occurs for type K thermocouples at around 185 °C.
41
 They operate very well in oxidizing atmospheres. If, however, a mostly reducing
atmosphere (such as hydrogen with a small amount of oxygen) comes into contact
with the wires, the chromium in the chromel alloy oxidizes. This reduces the emf
output, and the thermocouple reads low. This phenomenon is known as green rot,
due to the color of the affected alloy. Although not always distinctively green, the
chromel wire will develop a mottled silvery skin and become magnetic. An easy way
to check for this problem is to see whether the two wires are magnetic (normally,
chromel is non-magnetic).
Hydrogen in the atmosphere is the usual cause of green rot. At high
temperatures, it can diffuse through solid metals or an intact metal thermowell. Even
a sheath of magnesium oxide insulating the thermocouple will not keep the hydrogen
out.
Green rot does not occur in atmospheres sufficiently rich in oxygen, or oxygen-
free. A sealed thermowell can be filled with inert gas, or an oxygen scavenger (e.g. a
sacrificial titanium wire) can be added. Alternatively, additional oxygen can be
introduced into the thermowell. Another option is using a different thermocouple type
for the low-oxygen atmospheres where green rot can occur; a type N thermocouple is
a suitable alternative.
Type M
Type M (82%Ni/18%Mo–99.2%Ni/0.8%Co, by weight) are used in vacuum
furnaces for the same reasons as with type C (described below). Upper temperature is
limited to 1400 °C. It is less commonly used than other types.
Type N
Type N (Nicrosil–Nisil) thermocouples are suitable for use between −270 °C and
+1300 °C, owing to its stability and oxidation resistance. Sensitivity is about 39 µV/°C
at 900 °C, slightly lower compared to type K.
Designed at the defense Science and Technology Organization (DSTO) of
Australia, by Noel A. Burley, type - N thermocouples overcome the three principal

42
characteristic types and causes of thermoelectric instability in the standard base-metal
thermoelement materials.
A gradual and generally cumulative drift in thermal EMF on long exposure at
elevated temperatures. This is observed in all base - metal thermoelement materials
and is mainly due to compositional changes caused by oxidation, carburization, or
neutron irradiation that can produce transmutation in nuclear reactor environments.
In the case of type-K thermocouples, manganese and aluminum atoms from the KN
(negative) wire migrate to the KP (positive) wire, resulting in a down-scale drift due to
chemical contamination. This effect is cumulative and irreversible.
A short-term cyclic change in thermal EMF on heating in the temperature range
about 250 – 650 °C, which occurs in thermocouples of types K, J, T, and E. This kind of
EMF instability is associated with structural changes such as magnetic short-range order
in the metallurgical composition.
A time - independent perturbation in thermal EMF in specific temperature
ranges. This is due to composition-dependent magnetic transformations that perturb
the thermal EMFs in type - K thermocouples in the range about 25 – 225 °C, and in
type J above 730 °C.
The Nicrosil and Nisil thermocouple alloys show greatly enhanced
thermoelectric stability relative to the other standard base-metal thermocouple alloys
because their compositions substantially reduce the thermoelectric instabilities
described above. This is achieved primarily by increasing component solute
concentrations (chromium and silicon) in a base of nickel above those required to
cause a transition from internal to external modes of oxidation, and by selecting
solutes (silicon and magnesium) that preferentially oxidize to form a diffusion-barrier,
and hence oxidation-inhibiting films.

43
Type T
Type T (copper – constantan) thermocouples are suited for measurements in
the −200 to 350 °C range. Often used as a differential measurement, since only copper
wire touches the probes. Since both conductors are non-magnetic, there is no Curie
point and thus no abrupt change in characteristics. Type - T thermocouples have a
sensitivity of about 43 µV/°C. Note that copper has a much higher thermal conductivity
than the alloys generally used in thermocouple constructions, and so it is necessary
to exercise extra care with thermally anchoring type-T thermocouples. A similar
composition is found in the obsolete Type U in the German specification DIN
43712:1985-01.
- Fiberglass Tape Heater
Fiberglass Tape Heater are flexible heaters that are ideal for heating
columns, pipes, valves and transfer lines, especially when these applications need to
be observed. They can be applied to metal pipes as well as glassware.

Figure 33. Fiberglass Tape Heater

Fiberglass Tape Heater have an element wound on a fiberglass core and
covered in a braided glass fiber outer sheath; additionally, has a braided earth (ground)
wire beneath the outer sheath. They are available in different lengths to accommodate
a broad range of temperatures up to 450°C. The use of an energy or temperature
controller is recommended.

44
 - Relief Valve (Needle Valve)

Figure 34. Needle valve and cross section

A needle valve is a type of valve which can be used to regulate flow of
a substance, usually either gas or water, through an appliance or system. The unique
feature of the value is the inclusion of a small plunger, with a shape akin to a needle.
The plunger features a small handle, known as a handwheel, to enable easy and
precise turning of the valve. When fully attached, the elongated end of the valve fits
exactly into what is known as the seat, a part of the appliance that is being regulated.
However, if the valve is turned, space opens up between the needle and the seat,
allowing a minimal amount of substance to pass through. One design feature of most
needle valves dictates that a considerable number of turns are required to make even
a small amount of space open up. This enables gradual, accurate and precise control
over the amount of liquid/gas that can pass through the valve. Additionally, this can
prevent damage to gauges which could be affected by sudden bursts of liquid/gas,
and allows for better control and regulation in general. Some types of needle valves
are connected to an automated system and do not require manual regulation. These
will either operate on timers or respond to external data to regulate the closure and
opening of the valve as appropriate. These can be found in many types of engines and
gas piping. This allows for the operation of the valve to be optimal for the substance
and system that it is required for and will likely reduce the chances of damage through
incorrect operation of the valve.

45
 Needle valves are commonly made of robust and durable materials,
such as copper or steel. However, valves made from plastic and brass are sometimes
used depending on the specific requirements of the valve. Needle valves are used in
many different systems and applications, often featuring in carburetors. They can also
be found in some water heaters, used to regulate pressure inside a device. This can
also ensure that the appliance is running at maximum efficiency, without excess water
being used. In larger scale usage and delivery to numerous consumers, needle valves
can be used to regulate delivery of a product and relieve pressure on the systems
used to distribute the relevant substances. Needle valves are also sometimes used in
vacuum systems, in order to release a controlled yet steady supply of gas without a
great amount of pressure. The valve allows supply of gas to be slowed down
considerably before being shut off. This can minimize stress and strain on internal
machinery and components.
- Relay (Voltage)
A relay is an electrically operated switch. It consists of a set of input
terminals for a single or multiple control signals, and a set of operating contact
terminals. The switch may have any number of contacts in multiple contact forms,
such as make contacts, break contacts, or combinations thereof.

Figure 35. Voltage relay

Relays are used where it is necessary to control a circuit by an independent
low-power signal, or where several circuits must be controlled by one signal. Relays
were first used in long-distance telegraph circuits as signal repeaters. they refresh the

46
signal coming in from one circuit by transmitting it on another circuit. Relays were used
extensively in telephone exchanges and early computers to perform logical operations.
- Liquid crystal display (TM1637 Display)

Figure 36. TM1637Display

A liquid-crystal display (LCD) is a flat-panel display or other
electronically modulated optical device that uses the light-modulating properties of
liquid crystals combined with polarizers. Liquid crystals do not emit light directly,
instead using a backlight or reflector to produce images in color or monochrome. LCDs
are available to display arbitrary images (as in a general - purpose computer display)
or fixed images with low information content, which can be displayed or hidden, such
as preset words, digits, and seven-segment displays, as in a digital clock. They use the
same basic technology, except that arbitrary images are made from a matrix of small
pixels, while other displays have larger elements. LCDs can either be normally on
(positive) or off (negative), depending on the polarizer arrangement. For example, a
character positive LCD with a backlight will have black lettering on a background that
is the color of the backlight, and a character negative LCD will have a black background
with the letters being of the same color as the backlight. Optical filters are added to
white on blue LCDs to give them their characteristic appearance.

47
 Chapter 3 Methodology
3.1 Procedure

Flow chart below show the procedure of this project, start from conceptual
design until complete the actual prototype which contain 2 main sections (Vessel
and controller).

Start Project

Conceptual Design

Vessel Calculation Controller

No 3D CAD
Tinput

Material
Tinside < Tinput

Yes
Yes

Machining No
Heater ON

Heater OFF

48
 3.1.1 Conceptual Design
CO2 supercritical extraction machine for commercial used is expensive
because the machine is composed of many components such as CO2 tank, extraction
vessel, separator and recirculation equipment, these things make the device expensive.
This project purpose to make the device cheaper and reduce size to be portable
therefore, reducing vessels from 3 vessels to only one left. But since it's a concept we
have to experiment to find out the possibility that this new design can extract the oil.
- First Consideration

Figure 37. The process of CO2 Extraction by using 3 vessels

This design contains 3 vessels, CO2 tank will load CO2 to extraction vessel
which contain the specimens. CO2 soak with the specimen in the vessel after 1 hour it
will go to collection vessel in order to separate oil and CO2. This design is still costly
because only pump and recirculation equipment removed so no significant difference
from the commercial machine.

3.1.2 Shop for Design

To minimize the size of extraction machine and cost for local use which is
not necessary, need to be cut off such as collection vessel and separator but still
remain in function. So, the new design remains only extraction vessel that work as 3
in 1 vessel (CO2 tank, Extraction vessel, separator)

49
 Figure 38. The process of CO2 Extraction non-recirculated CO2
3.1.3 Machine Assembly
We heated the system up with heater. When solid CO2 are in close volume.
The temperature is rising up, the pressure is rising up too (PV = nRT). Solid CO2 change
the phase to super critical point (71 Bars, 31°C) but we need to wait the time until we
get the best condition of extraction depend on the types of raw material. We soak the
raw material inside vessel (1-2 hour). Turn the position into start point and blew the
pressure to ambient when finished installation.
1. Install bottom flange with stud, locked bolt, bottom bolt and washer then
place it on holder stand.
2. put the reactor vessel (800 ml) in the middle of bottom flange and stud then
we assembly heater with reactor.
3. Put the raw material (50 g) in the capsule and hang with head flange for ready
to close the vessel.
4. Put the solid carbon dioxide (400 g).
5. Put the head flange, head bolt and washer for close the reactor.
6. Close the frame on the holder stand for lock the extractor then use torque
wrench to close to head bolt.
7. Use pound torque to check (we require 100 ponds for every head bolt).
8. Set the temperature as we want.

50
 9. Turn on heater and thermocouple. Heat it up to supercritical point and
condition point (the extraction process take 1 hour).
3.1.4 Experiment

3.2 Material & Equipment

3.2.1 Software
Software use to design the prototype for visualization and construction
to know the exact dimension and able to revise if there is a mistake before
machining.
- Solid Work (Mechanical Design)

Figure 39. Solid work software

51
 - Fritzing (Electrical Design)

Figure 40. Temperature Control Unit (Schematic)

3.2.1 Material & Tools

- Carbon seamless steel pipe (Di = 32 mm, Do = 100 mm)
- Blind flange (JIS 10K)
- Stud (Threaded rod)
- O-ring (D = 80 mm, Tmax = 120 °C)
- Pressure Gauge (400 Bar)
- Microcontroller (Arduino)
- Thermocouple (Type K)
- Relief Valve (Needle Valve)
- Relay (Voltage)
- Liquid crystal display (TM1637 Display)

52
 Chapter 4. Result

4.1 Designing Model

The supercritical CO2 Extraction vessel is designed to able to operate at high

pressure about 400 bar so the material used to make the vessel must be strong and
can endure the pressure. Therefore, before designing we need to know what material
has appropriate properties that can deal with it.
From the calculation of thick wall cylinder.

Figure 41. Design Model

Design Condition
Inside pressure outside pressure Inside radius outside radius radius to point
(MPa) (MPa) (mm) (mm) in the wall (mm)
40 0 32 50 32

Result
Axial stress (MPa) Circumferential stress (MPa) Radial Stress (MPa)
27.8 95.5 -40

According to the calculation we decided to use carbon seamless steel pipe

which has enough strength to resist high pressure.

53
 4.1.1 CAD Modeling
The first process before start machining is to model 3D CAD by using Solid
Work to know the exact dimension of the prototype for visualizing and construction.
The figure below shows the final design of supercritical CO2 extraction. By using steam
pipe as a vessel and Its inside diameter is 3.2 cm, outside diameter 30 cm. and 25 cm.
tall (volume = 804.24 cm3). Dry ice and specimen will be put inside and will be heated
to the critical point (73 bar and 31°C). Insert O-ring in the gap between vessel and flank,
O-ring acts as a gasket to prevent leakage from high pressure because the steel contact
can’t seal it tightly. Flank is closed in the both side of vessel and fastened with 8 studs
to make sure that it’s strong enough and will get exploded.

Figure 42. CAD Model

The measurement tools (pressure gauge, thermocouple and relief valve) are
attached at the top of the vessel, these tools are used to inspect the phase of CO2 as
well as to measure temperature inside the vessel because thermocouple works related
to heater by using thermostat control.
The stand (Figure 43) is used to place the vessel above the dish and it can
rotate 360 degree along x - axis, rotating the vessel is to study the mixture possibility
of CO2 and raw material will get the better. Wheels are attached to make it more
portable.

54
 Figure 43. Stand holder (360 degree rotate)

4.2 Actual Model

The actual model after machining was machined by our design although some
dimension was changed a little bit and sight glass used to inspect supercritical CO 2
phase was not installed due to unable to find part but there is no significant effect to
the extraction vessel itself because it was designed as over specification.

Figure 44. Extraction Vessel

55
 Figure 45. Extraction vessel on stand holder
Stand holder is designed able to rotate the extraction vessel for mixture of
solvent and raw material due to solid CO2 is put under the specimen, rotating the
stand for soaking it evenly.

Figure 46. Extraction vessel that contain CO2 and specimens (inside)

56
4.3 Control Unit (Thermostat ON/OFF)

Figure 47. Actual Control Unit on board

Control Unit, use Arduino as a processor connect with other components to
control temperature and display temperature inside the vessel on LCD for inspection
for real time.

4.4 Result of Experiment

Figure 48. Pressure and Temperature reach the critical point after operate for 20
minutes.

57
 Figure 49. Show temperature and pressure when the prototype operated
Figure 48 show the result of the experiment when the prototype was operating,
temperature and pressure were plotted in a graph comparing with CO2 phase diagram.
Dry ice was changed from solid to supercritical state when reach critical point after
operating time 20 minutes (Figure 50).

250 230
222 220
209 215
200
190
200 180
170
161
150
Pressure (Bar)

139
150 128
115
100
100 88
75
62
49
40
50

0
0
0 5 10 15 20 25 30 35 40 45 50 55 60 65 70 75 80 85 90 95 100
Time (Minute)

Figure 50. Pressure increases with time

58
 140
125 128
121
116
120 112
106
100
95
100 89
Temperature (°C)
83
77
80 70
64
57
60 50
43
36
40 30
21 19
20
7

0
0 5 10 15 20 25 30 35 40 45 50 55 60 65 70 75 80 85 90 95 100
Time(Minute)

Figure 51. Temperature increases with time

Figure 52. Oil remain on the valve’s surface

From the experiment when relief the pressure inside the vessel (Temperature
= 105 °C, Pressure = 200 Bar) oil came out with carbon dioxide and it stuck around the
valve. Some oil left on the surface inside the vessel and it need to be squeezed to
get the remaining oil.

59
 Figure 53. Oil stains on the container (left) and remain inside the vessel (right)

4.5 Result & Discussion

The supercritical carbon dioxide extractor (Close loop system) utilized in the
experiment is able to extract essential oil but in very low amount and unquantifiable
its volume. Due to each plant has different condition in extraction and withal the
extracted oil emerges when open valve to blow the pressure. A container is needed
to cover the valve to amass oil, some oil remains at the valve’s surface in (Figure 53)
but still visualize. The factor causes low quantity of oil due to the machine can control
only temperature (from heater) result insufficient pressure to extract raw material at
its condition such as in extraction of coffee, the appropriate point is about 80 °C, 300
Bar but at this temperature the machine was running at 155 Bar. The pressure and
temperature quantified during experiment shown in Figure 49. From the experiment
the extracted oil has high viscosity, concentration, smell is vigorous and withal long -
lasting.

60
 Chapter 5 Conclusion
5.1 Summary

At the commencement, the researcher was studying the process of extraction,

high pressure vessel designing, matching the material, thermodynamic property of
carbon dioxide and CAD design drawing. After the prototype was consummated
(portable CO2 supercritical extractor) and (non- circulated carbon dioxide) the concept
of SFE was verified and done experiment with raw material (coffee, Bergamot,
Mangosteen peel). From the experiment paramount oil were not found but the
conspicuous of oil are in the form of scent and the wax around the relieving valve.

5.2 Future Work

5.2.1 Problem Found

- Design and Machining
Due to the fact that we don’t know the exact value of yield from
extraction process so we design the volume of vessel is 800 ml by utilizing AISI 1024
(seamless pipe) as material for abbreviating cost and can resist pressure but the
problem is the rust inside vessel. It can load solid carbon dioxide around 400 g and
raw material 50 g in capsule that hang with Head Flange. We are able to control
temperature inside vessel (0 - 120 °C) and pressure (40 – 220 Bar). We design for over
specification as safety reason. But this machine didn’t good culminating surface inside
vessel. At the initial experiment leak are found around relief value screw (Figure 55),
during extraction processing, the oil came out from the leak so the yield is very low.

61
 Figure 54. Leak around assuagement value screw

- Equipment and Controller

The extractor prototype can quantify pressure and temperature but
cannot control at very high pressure (more than 250 Bar) as appropriate condition. So,
installation of pump and controller can control the pressure to the condition but need
more cost. Only temperature control also can extract the oil.
- Assembly
From the design, opiating AISI 1024 as material, so the extractor is very
cumbersomely hefty and weldless designing, for the safety reason so the component
of extractor needs to assembly every time with studs and bolts. requirement of time
to assembly around 15 minutes and need 2 people to assembly, for people who want
to do this prototype the suggestion is redesign for more convenience to utilize and
rapid assembly.
- Raw Material, Solid Carbon dioxide, O - Ring
Requirement of raw material need to be grinded as powder for more
yield but with our grinder cannot done as powder.

62
 Buying many times of solid carbon dioxide (1 kg = 30 baht) because it
can facilely to sublimate in economic reason it is not worth when compere with close
loop system (Circulated Carbon dioxide). Total the researcher bought 35 kg of solid
carbon dioxide (1,050 baht).
The rubber O–ring cannot resist at the highest condition point
(120°C,220 Bar) because it resists only at 100 °C, 200 Bar.

5.3 Recommendation

1. The heat is affected by the heat accumulation of the thick extraction vessel,
making the temperature control need to be set to a lower than the genuine value, it
is compulsory to compensate for the signal. So that the sensor can signal the correct
value.
2. Change the material to food grade material (stainless 304, 314, 316).
3. Redesign to close loop system (Circulated carbon dioxide) for more value
cost. Redesign for immensely colossal scale extraction and more better machining to
get more essential oils. but need to integrate more equipment and budget (Pump,
Condenser, Vessel, High pressure pipe).
4. Redesign for more convenient to utilize and assembly.
5. Change rubber O-ring (resist 120 °C and 200 Bar) to aluminum O-ring for more
pressure resists.
6. This extractor can operate with low condition raw material (Tmax = 100 °C,
Pmax = 220 Bar) such as Rose, Bergamot, Butterfly flower and Lotus.

7. After the experiment, when relieving carbon dioxide from extraction vessel.
suggestion to do in open - air area or ventilated air because carbon dioxide can make
you dizzy from breathing.
8. More study and design for oil separator vessel.
9. Install observe sight glass for more understanding of supercritical fluid
behavior.

63
 Reference
[1] Evid Based Complement Alternat Med. 2014; 2014: 467363. Published online 2014
Jun 22. Doi: 10.1155/2014/467363
[2] Selected commercial plants: A review of extraction and isolation of bioactive
compounds and their pharmacological market value, Jayanta Kumar Patra, Gitishree
Das, Siyoung Lee, Seok-Seong Kang, Han-Seung Shin
[3] Cold press in oil extraction, Büşra Çakaloğlu, Vasfiye Hazal Ozyurt, Semih Otles,
December 2018 DOI: 10.24263/2304-974X-2018-7-4-9
[4] Green Analytical Chemistry, M.de la Guardia, S.Armenta, in Comprehensive
Analytical Chemistry, 2011
[5] Juliana M. Prado, Smain Chemat, Conventional extraction in Food Waste Recovery,
2015
[6] A Comprehensive guide to essential oil extraction methods, March, 2017
www.newdirectionsaromatics.com/blog/articles/how-essential-oils-are-made.html
[7] Mass Spectrometry for Natural Product Discovery, Katherine B. Louie, ... Trent R.
Northen, in Reference Module in Chemistry, Molecular Sciences and Chemical
Engineering, 2020
[8] Preparation, Standardization, and Quality Control of Medicinal Plants in Africa, M.O.
Nafiu, ... S.B. Adeyemi, in Medicinal Spices and Vegetables from Africa, 2017
[9] Q. Wang, L. Liu, L. Wang, Y. Guo, J. Wang in Peanuts: Processing Technology and
Product Development, 2016
[10] Water requirement and sustainability of textile processing industries, A.S.M. Raja,
A. Arputharaj, Sujata Saxena, P.G. Patil in Water in Textiles and Fashion, 2019
[11] Pressurized Liquid Extraction of Contaminants from Environmental Samples,
Antonio Nieto, Francesc Borrull, Rosa Maria Marcé, Eva Pocurull, April 2008

64
 Reference
[12]www.chem.libretexts.org/Bookshelves/Physical_and_Theoretical_Chemistry_Textb
ook_Maps/Supplemental_Modules_(Physical_and_Theoretical_Chemistry)/Physical_Pr
operties_of_Matter/States_of_Matter/Phase_Transitions/Phase_Diagrams
[13] Research and Development on Components Natural oil Extractor with Supercritical
carbon dioxide Technique (SC-CO2) and Combination Mixer Magnetic Dr. Pinit Jirukakul
2019, Department of Agricultural
[14] Volatile Oil Extraction Using Supercritical Fluid ผศ.ดร.ภก. ธนภัทร ทรงศักดิ์ กลุม่ วิชา
เภสัชเวท คณะเภสัชศาสตร์ มหาวิทยาลัยรังสิต
[15] https://luxatic.com/top-10-most-expensive-essential-oils-in-the-world-done
[16] Microwave-Assisted Extraction Emilie Destandau, Thomas Michel, Claire Elfakir,
January 2013, RSC Green Chemistry

65
Appendices

66
 Appendix - A
Arduino Code (Thermostat ON/OFF)
#include "max6675.h"
#include <Arduino.h>
#include <LiquidCrystal.h>
int thermoDO = 4;
int thermoCS = 5;
int thermoCLK = 6; // code for display
#define CLK 2
#define DIO 3
#define TEST_DELAY 2000
TM1637Display display(CLK, DIO); // code for display end
MAX6675 thermocouple(thermoCLK, thermoCS, thermoDO);
int vccPin = 3;
int gndPin = 2;
double Setpoint, PV;
double Error;
void setup () {
Serial.begin(9600); // use Arduino pins
pinMode(vccPin, OUTPUT); digitalWrite(vccPin, HIGH);
pinMode(gndPin, OUTPUT); digitalWrite(gndPin, LOW);
pinMode(10, OUTPUT);// set pin 10 as output
Serial.println("Robojax: MAX6675 test"); // wait for MAX chip to stabilize
delay(500); }
void loop() {
display.setBrightness(0x0f); // All segments on
67
 uint8_t data[] = { 0x0, 0x0, 0x0, 0x0 };
display.setSegments(data);
delay(1);
int temp = (int) thermocouple.readCelsius();
display.showNumberDec(temp, true, 3, 0);
Serial.print("C = ");
Serial.println(thermocouple.readCelsius());
Serial.print("F = ");
Serial.println(thermocouple.readFahrenheit());
Setpoint = 70;
PV = thermocouple.readCelsius();
Error = thermocouple.readCelsius()-70;
if(Error>0)
{
digitalWrite(10, LOW);// set pin 10 LOW
Serial.print("OFF");
}
else if(Error<0)=
{
digitalWrite(10, HIGH);// set pin 10 LOW
Serial.print("ON");
}
delay(1000);
}

68
 Appendix - B
Budget
Index List units Price (Bath)
Electrical Arduino UNO R3 1 300-
Fiber Heater 1 300-
Max6675 1 90-
TM1637Display 1 40-
Relay 1 80-
Mechanical Extraction Vessel 1 1,000-
Stud 8 300-
Bolt 24 180-
Washer 24 60-
O-Ring 16 480-
Flange 2 400-
M28 Wrench Block 2 330-
Relief Vale 1 1,760-
Pressure Gage 1 600-
Thermocouple 2 1,284-
Thermometer 1 370-
Nipple 2 360-
Machining Cost 1 3,000-
Mylar 2 200-

69
 Index List units Price
Torque Wrench 1 300-
T-Wrench 1 400-
Lock Wrench 1 230-
Holder Stand 1 500-
Wheels 4 300-
Color 2 200-
Grooves 2 170-
Etc. Raw Material 1 kg 400-
Ice Box 1 200-
Solid Carbon Dioxide 35 kg 1,050-
Grinding Machine 1 400-
Stainless Capsule 1 300-
Syringe 10 120-
Total Cost 15,434-

70
 Appendix - C
Top 10 most high value essential oil in Global market
1. Champaca Absolute Essential Oil

Used for centuries as a great way to cure depression and relieve stress, vertigo
or headaches, the Champaca Absolute Essential Oil seems to be one of the best when
it comes to medicinal purposes. It has regenerative properties, helping with wounds
from acne, spots, wrinkles and complexions. Its powerful citrus and floral scent is much
appreciated in India and parts of Asia where it’s also used as a perfume and as a
powerful aphrodisiac. A very expensive one, since the price per ounce is a staggering
$2,256, making it the most expensive essential oil in the world.

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 2. Tuberose Absolute Essential Oil

The Tuberose is a perennial plant cultivated in Mexico with extracts of it used

in perfumery. Its oil is extracted by infusing the petals in palm oil, separated afterwards
from the tuberose essence through the process of evaporation. The Tuberose Absolute
Essential oil is considered luxurious oil and it’s used in aromatherapy for or in
fragrances. The relaxation properties make it a great help against insomnia, though
some use it for inspiration purposes and even as an aphrodisiac. Whatever the use,
make sure it’s worth it, since an ounce of this oil costs a great $1,645.

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 3. Fragipani Absolute Essential Oil

The Frangipani flower is a rare species, found only on the Comoros Islands in
France. The oil extract is very thick and has an intense sweet floral fragrance, with hints
of exotic spices, making it a main component of high-class perfumery. Besides
perfumes, the Frangipani Absolute Essential oil has medicinal uses as well, reducing
stress and inflammations. The price for an ounce of this oil reaches a staggering $1,482.

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 4. Cannabis Flower Essential Oil

Now here’s an interesting one, the Cannabis Flower Essential oil, also known
as hemp essential oil. Its main use is in cosmetics, perfumes, soaps and candles for its
pleasant, relaxing smell. It’s used as well to flavor some foods or beverages. The plant
itself, though is known to have medicinal uses, like alleviating inflammations, skin
irritations or hormonal imbalances, it’s highly regulated so growing it in many parts of
the world is illegal. That’s what makes it very popular to some and the oil extracted
from it so expensive with a price of $946 per ounce.

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 5. Agarwood Essential Oil

The Agarwood Essential oil, also known as Oud oil, it’s an extremely rare and
much appreciated oil for its great aroma and medicinal uses. As the name states, it’s
extracted from the agarwood, which is listed as a potential threatened species, making
it one of the most expensive raw materials in the world. The trees require a long time
to grow and they’re found only in isolated regions of countries like India, Bhutan,
Vietnam, Indonesia, Papua New Guinea and a few others. The sweet, woody fragrance
of the oil is praised so much that the price for an ounce of this oil goes to $850.

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 6. Rose Essential Oil

Who doesn’t know roses and all those commercials involving beautiful ladies,
perfumes and rose petals? They’re everywhere. Well, it’s true. At least the part with
the rose petals, since they are highly prized in the perfume industry and are widely
used around the world. The Rose Essential Oil is extracted from two types of rose
petals, the ottos and the absolutes, using around four tons of petals for every pound
of oil extracted. Sounds crazy, right? Well, the flavor of this oil is very intense. The
same thing can be said about its price. You can buy it for a good $700 per ounce.

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 7. Seaweed Absolute Extra essential oil

The Seaweed Absolute Extra Essential Oil is made as the name says, from
seaweed, one that is found on the coasts of the North Sea, the Baltic sea and the
Atlantic and Pacific Oceans. First the original source of iodine, with its salt-water, moss,
green herbs and undertones of leather in its aroma now it’s the main choice for natural
perfumes. The Seaweed Absolute Extra essential oil is the main ingredient in these
kinds of perfumes and it’s also used for skin care products, but its price rises to a high
$650 per ounce.

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 8. Elecampane Essential Oil

The Elecampane Essential oil comes from a plant in the sunflower family
known as well as horse heal, which grows in Europe, Asia and some parts in North
America. The plant was considered sacred by the Celts and its name and history goes
back to Helen of Troy. More than that, it’s one of the ingredients used to create
absinthe, so it does have an important role in the world besides perfumes and
essential oils. It’s also one of the rarest in the world. we suspect absinthe to be the
cause for that and its essential oil is as well used in herbal medicine as an expectorant
or for water retention. One ounce of this oil costs $560.

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 9. Sandalwood Essential Oil

The Sandalwood Essential oil is extracted by steam distillation from the chips
of the wood with the same name. Used in perfumes, cosmetics and Ayurveda
medicine, the oil is praised by many. The sandalwood is the second most expensive
tree in the world, so you can expect the price of the oil to be high. More than that,
the process is a very complex one and the fact that it’s produced only in India makes
this oil scarce. Its price per ounce is $492.

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 10.Neroli Essential Oil

In 17th century there was a princess, Anne Marie Orsini, princess of Nerola, Italy.
She was the first one to introduce the oil made from the blossom of the bitter orange
tree, hence the name of the oil today. It has a honey-like sweetness to it with some
spicy tones and it’s used very much in perfumes. We don’t know if the cause is wearing
a princess name or not, but the price for an ounce of this essential oil is a huge $354.
We know that the sum doesn’t sound too much, but it’s just an ounce. Almost nothing.
Some sources even claim that this oil is one of the secret ingredients in Coca Cola.

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 Appendix - E
Thai herb essential oil

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 Appendix - F
Benefits and Uses of Coffee Essential Oil
1. Stimulate Hair Growth
Many people have sought out alternative methods of restoring their hair or
saving what hair may be remaining. Traditional therapies prescribed by the medical
community may have no effect and end up being costly to implement. There is also
the issue of using chemicals, which may affect the body in other, unforeseen, ways.
The caffeine found in coffee essential oil has been found to counteract testosterone
caused hair thinning. They believe it stimulates the follicles, allowing for more activity
and longer hair.
2. Disinfectant
Whenever cold and flu season hits, we usually turn to bleach wipes to help
keep us germ-free. However, there are new strains of common diseases that have
become resistant to medical intervention, but still, respond to natural considerations.
Coffee oil has many properties such as being antibacterial. You can add a couple drops
to vinegar to create a surface spray that will help keep your house clean and reminding
you of a fresh cup of coffee at the same time.
3. Reduce Cellulite
This seems to be a persistent problem for many people, despite changes in
diet and exercise. Your body is determined to hold onto the lumpy bulges on the hips
and thighs. Research has shown that using coffee infused oil for cellulite does show a
change in the appearance of cellulite on the body. Mix the coffee oil with carrier oil
and apply it anywhere on your body where you have cellulite. All the beneficial
chemicals will be absorbed through your skin, and you may begin to see changes in
your body.

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 4. Regulate Mood
One of the compounds found in coffee essential oil also has a slightly sedative
effect, which can be helpful when it comes to dealing with the extremes of depression
and other mental disorders. This effect allows the mind and body to relax so that
hormones can be balanced between feeling good and existing in a constant state of
stress. Add coffee essential oil to your diffuser when you need to be relaxed. Coffee
essential oil blends well with ylang-ylang, which is also a mood enhancer with a slight
floral smell that shouldn’t overwhelm the smell of coffee, or sandalwood if you prefer
a less citrus scent.
5. Skin Care
When you think of coffee, skin cleanser is likely the last thing you would think
of when considering how to use coffee infused oil. It has been shown that using this
oil mixed with a carrier and used as a topical application can help prevent the signs of
aging, which are usually indicators of the cells being damaged by free radicals in the
environment. Add some coffee oil to witch hazel to add in the astringent properties
found in it. The oil will sink into your skin and work to protect you from further damage.
6. Boosts Your Immune System
Coffee is one of the biggest sources of antioxidants for the Western world, and
coffee essential oil comes packed full of antioxidants that can boost your immune
system. Several studies have highlighted how coffee’s properties can help prevent free
radical damage to your cells and reduce your oxidative stress. This can boost your
immune system and keep you healthier.

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Benefits and Uses of Bergamot Essential Oil
1. Ease Anxiety and Depression
We spend most of our waking hours surrounded by stressful environments:
meetings, project deadlines, coworkers, and family obligations. We are in constant
contact with the world, and many of us find it hard to switch off even in our downtime.
This can lead to bouts of anxiety or depression. Our body responds to the stress with
the hormone cortisol but does not process this or may even overproduce this due to
a constant state of stress. Bergamot essential oil has been shown to reduce the
production of cortisol as well as the inflammation which occurs that prevent the brain
from processing stress hormones properly. It allows your body to relax and eases the
effects of constant stress.
2. Improve Skin Health
There are as many different causes of skin issues as there are types of skin
problems. Many times, the treatment for an issue causes undesirable side effects in
other areas of the body, and traditional medications may alleviate some symptoms
but still require some additional assistance in clearing the conditions completely.
Bergamot essential oil has been proven to treat both bacterial and fungal skin
conditions, killing bacteria and fungus and reducing inflammation of the skin. This
allows wounds or open sores to heal faster. These properties also make it one of the
effective essential oils for hair growth. Mix a few drops of bergamot and lemon with
witch hazel for a natural cleanser to help kill the bacteria found in acne and heal
inflamed acne sores.
3. Fight Infections
This particular property comes in handy if you want to have a clean home but
would also like to prevent the possible occurrence of resistant bacteria and virus that
can be created when using traditional cleaning products. They are full of chemicals
that can not only strengthen germs but may also be dangerous to use in your home.
Bergamot oil has proven antibacterial and antifungal properties, which can be used to
prevent foodborne illnesses caused by bacteria such as e. coli and staphylococcus.
You may also decrease airborne sickness by killing bacteria and molds that float around

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your home, causing respiratory issues. Make your own household cleaner with
bergamot, lemon, vinegar, and water. Spray on your hard surfaces to prevent
transmission of germs. You can also use in a diffuser with eucalyptus to not only
prevent respiratory illness but ease symptoms as well.
4. Lower Blood Pressure
Along with alleviating stress and depression, bergamot essential oil can also
help lower blood pressure. Blood pressure can be related to other diseases such as
heart disease, which is the number one cause of death. Elevated blood pressure is the
result of several different causes stress or arterial inflammation. Bergamot oil has been
proven to reduce blood pressure by relieving stress and cortisol levels and improve
vascular flexibility. Create your own stress-relieving diffuser mix with bergamot,
lavender, and ylang-ylang for anti-inflammatory and relaxing properties.
5. Relieve Cold Symptoms
No matter how we might wish for a cure for the common cold, it seems like
that is still a distant dream. However, there may be natural ways to help ease the
symptoms of a cold such as fever and coughing. Using bergamot essential oil in an
essential oil recipe for colds may aid in recovery time by helping to reduce inflamed
respiratory tissue and inflammation in the body which triggers the body’s response in
the form of a fever. Using this oil as part of essential oil diffuser recipes for colds may
not cure you, but it can be used in conjunction with other over-the-counter
medications to help ease further symptoms and aid in a faster recovery. Use a mix of
bergamot and other cold fighting oils such as eucalyptus, peppermint, or lemon. These
oils share many of the same properties and may be used as a complement to your
other symptom-relieving therapies.
6. Reduce Cholesterol
When visiting the doctor, you may be subjected to a cholesterol check to
examine the amount of good and bad cholesterol, which allows your health
practitioner to keep an eye on the lipid level of your blood and catch any possible
complications before they arise. Bergamot has been shown to have an impact on the
lipid level of your blood and may even increase the good cholesterol levels. This is

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due to the number of flavonoids and the high linalool content found in bergamot.
Bergamot may be used as a complementary therapy to any medications that have
been prescribed by your health care provider.

Benefits and Uses of Mangosteen Peels Essential Oil

Among the powerful phytonutrients found within the rind of the mangosteen,
xanthones stand alone in their spectacular edges. Scientific studies counsel xanthones
might promote healthy organic process. The entire mangosteen fruit, jam-choked with
present xanthones, may help: Maintain enteral health, Support the system, neutralize
free radicals, facilitate support animal tissue and joint operate, Promote a healthy
seasonal system respiratory,
Healthy Island Mangosteen helps support. All the best edges of the
mangosteen fruit is that it strengthens the body’s system. By drinking it daily, your
body’s system is optimized to retort against the invasion of out of doors germs,
bacterium and viruses because it fights them off and protects you from infection.
Xanthones found within the mangosteen additionally helps the system similarly
because the general wellbeing of the body and mind. Among the powerful
phytonutrients found within the rind of the mangosteen, xanthones stand alone in
their spectacular edges. Scientific studies counsel xanthones might promote healthy
organic process. The entire mangosteen fruit, jam-choked with present xanthones, may
help:
1. Maintain enteral health.
2. Support the system.
3. Neutralize free radicals.
4. Support animal tissue and joint operate.
5. Promote a healthy seasonal systema respiratorium.
The subsurface of the mangosteen excocarp will contain completely different
polyphenols that do embody xanthone and tannins. Xanthonoid could be a natural
chemical phenolic resin compound that’s fashioned from the xanthone backbone and
it’s a member of the family Clusiaceae family. Xanthone, itself, is AN compound, and

86
it’s used as each a pesticide, override for secret writing lepidopteran eggs, and
conjointly a chemical.
Tannins are a bitter plant compound that binds itself to proteins, amino acids,
and different alkaloids. The take leave the mangosteen is loaded with xanthonoids,
one in all that is mangostatin, and different key phytochemicals that have super anti-
oxidant properties in them.
There are variant studies done on the take leave the mangosteen and a few
superb findings were learned. From the juice, which comes directly from the
mangosteen peel, there are plenty of healthiness aspects.
Polyphenol – {a cluster|a gaggle|a bunch} of plant chemical substances
characterized by the presence of over one phenolic resin group. Polyphenols are
chargeable for the color of some plants and are thought of sturdy antioxidants with
potential health edges.
Flavonoid – over 5,000 present flavonoids are characterised from varied plants.
The helpful effects of plant-derived food are usually attributed to flavonoid
compounds, instead of glorious nutrients, as they show a large vary of biological
effects.
-Alpha mangostin Mangostinone
-Beta mangostin Garcimangosone A
-Euxaonthone Garcimangosone B
-Iso-mangostin Mangostanol
-Garcinone A Mangostenol
-Garcinone B Mangostenone A
-Garcinone C Mangostenone B
-Xanthone-B this is often a spa 8-desoxygartanin

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 Appendix - G
Thailand Import and Export Index

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 Appendix - H
Global Essential oil Market size

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 Appendix – I
Material Table

92
 Appendix - J
Bolt and Stud Table

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 Student Biographies
Name: Ritthikiat Churoop
Student ID: 5810545327
Address: 97/44 Ngamwongwan52,Ngamwongwan Road, Ladyao, Jatujak, Bangkok 10900
Mobile Phone: 062-363-0488
E-mail: ko.ritthikiat@gmail.com
Education High School: Saengthong Vittaya school

2.Name: Phanuwat Chaichutchouwakul

Student ID: 5910546163
Address:1555/127 The Editor Pahonyothin Road , SamsenNai, Phayathai, Bangkok 10400
Mobile Phone: 081-261-4157
E-mail: phanuwat.cha@ku.th
Education High School: Udonpittayanukul school

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